JP6776609B2 - Anisotropic conductive film - Google Patents

Anisotropic conductive film Download PDF

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Publication number
JP6776609B2
JP6776609B2 JP2016096768A JP2016096768A JP6776609B2 JP 6776609 B2 JP6776609 B2 JP 6776609B2 JP 2016096768 A JP2016096768 A JP 2016096768A JP 2016096768 A JP2016096768 A JP 2016096768A JP 6776609 B2 JP6776609 B2 JP 6776609B2
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Japan
Prior art keywords
conductive film
anisotropic conductive
evaluation
film according
particles
Prior art date
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JP2016096768A
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Japanese (ja)
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JP2017152354A (en
JP2017152354A5 (en
Inventor
慎一 林
慎一 林
憲司 徳久
憲司 徳久
恵津子 山口
恵津子 山口
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dexerials Corp
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Dexerials Corp
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Publication date
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Priority to KR1020247000952A priority Critical patent/KR20240010091A/en
Priority to CN201780010511.3A priority patent/CN108602970A/en
Priority to US16/071,858 priority patent/US10964440B2/en
Priority to KR1020237009590A priority patent/KR102624920B1/en
Priority to PCT/JP2017/004887 priority patent/WO2017145801A1/en
Priority to KR1020217013728A priority patent/KR102513546B1/en
Priority to KR1020187019787A priority patent/KR102363322B1/en
Priority to TW112117949A priority patent/TW202334315A/en
Priority to TW106104604A priority patent/TWI804460B/en
Publication of JP2017152354A publication Critical patent/JP2017152354A/en
Publication of JP2017152354A5 publication Critical patent/JP2017152354A5/ja
Priority to JP2020168219A priority patent/JP6973593B2/en
Application granted granted Critical
Publication of JP6776609B2 publication Critical patent/JP6776609B2/en
Priority to JP2021180149A priority patent/JP7421132B2/en
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Description

本発明は、異方性導電フィルムに関する。 The present invention relates to an anisotropic conductive film.

従来より、ＩＣチップなどの電子部品を配線基板に実装する際に、重合性化合物を含有する絶縁性のバインダ組成物に導電粒子が分散している異方性導電フィルムが広く用いられている。このような異方性導電フィルムには、低温速硬化性を実現するために、重合性化合物として、汎用のグリシジルエーテル系化合物よりもカチオン重合反応性の高い脂環式エポキシ化合物を使用すると共に、酸素による重合阻害がなく、暗反応性を示す重合開始剤として、熱によりプロトンを発生するスルホニウム塩系熱酸発生剤を使用することが提案されている（特許文献1〜３）。このような、脂環式エポキシ化合物とスルホニウム塩系熱酸発生剤とを含有する従来の異方性導電フィルムは、比較的低温（例えば１００℃程度）の硬化温度を示している。 Conventionally, when an electronic component such as an IC chip is mounted on a wiring board, an anisotropic conductive film in which conductive particles are dispersed in an insulating binder composition containing a polymerizable compound has been widely used. In such an anisotropic conductive film, in order to realize low-temperature rapid curing, an alicyclic epoxy compound having a higher cationic polymerization reactivity than a general-purpose glycidyl ether-based compound is used as the polymerizable compound, and the alicyclic epoxy compound is used. It has been proposed to use a sulfonium salt-based thermoacid generator that generates protons by heat as a polymerization initiator that does not inhibit polymerization by oxygen and exhibits dark reactivity (Patent Documents 1 to 3). Such a conventional anisotropic conductive film containing an alicyclic epoxy compound and a sulfonium salt-based thermoacid generator exhibits a curing temperature at a relatively low temperature (for example, about 100 ° C.).

特開平９−１７６１１２号公報Japanese Unexamined Patent Publication No. 9-176112 特開２００８−３０８５９６号公報Japanese Unexamined Patent Publication No. 2008-308596 国際公開２０１２／０１８１２３号International release 2012/018123

しかしながら、前述したような異方性導電フィルムについては、商取引の国際化等により製造から実使用までの時間が長くなるという問題や、また、空調が整備されていない倉庫で保管される場合があるといった問題があり、仮貼り性や圧痕等の観点からの保存安定性（保管ライフ性）の低下や、密着特性等の観点からの接続信頼性の低下が懸念されるようになっている。 However, the anisotropic conductive film as described above may have a problem that the time from manufacturing to actual use becomes long due to the internationalization of commercial transactions, and may be stored in a warehouse where air conditioning is not maintained. There are concerns about a decrease in storage stability (storage life) from the viewpoint of temporary sticking property and indentation, and a decrease in connection reliability from the viewpoint of adhesion characteristics and the like.

本発明の課題は、脂環式エポキシ化合物を使用するカチオン重合性の異方性導電フィルムに対し、従前と変わらない硬化温度と接続信頼性とを担保しながらも、今まで以上に優れた保管ライフ性を実現できるようにすることである。 An object of the present invention is to store a cationically polymerizable anisotropic conductive film using an alicyclic epoxy compound, which is more excellent than ever, while ensuring the same curing temperature and connection reliability as before. It is to be able to realize life.

本発明者は、カチオン重合性化合物として、脂環式エポキシ化合物に加えて低極性オキセタン化合物を特定割合で併用し、且つカチオン重合開始剤として、スルホニウム塩系熱酸発生剤に代えて第４級アンモニウム塩系熱酸発生剤を使用することにより、今までと変わらない硬化温度と接続信頼性とを担保しながらも、今まで以上に優れた保管ライフ性を実現できることを見出し、本発明を完成させるに至った。 The present inventor uses a low polar oxetane compound in a specific ratio in addition to the alicyclic epoxy compound as the cationically polymerizable compound, and as the cationic polymerization initiator, replaces the sulfonium salt-based thermoacid generator with a fourth grade. Completed the present invention by finding that by using an ammonium salt-based thermoacid generator, it is possible to realize better storage life than ever while ensuring the same curing temperature and connection reliability as before. I came to let you.

即ち、本発明は、成膜用成分とカチオン重合性成分とを含有するバインダ組成物と、カチオン重合開始剤と、導電粒子とを含有する異方性導電フィルムであって、
カチオン重合開始剤が、第４級アンモニウム塩系熱酸発生剤であり、カチオン重合性成分が、脂環式エポキシ化合物と低極性オキセタン化合物とを含有している異方性導電フィルムを提供する。 That is, the present invention is an anisotropic conductive film containing a binder composition containing a film-forming component and a cationically polymerizable component, a cationic polymerization initiator, and conductive particles.
Provided is an anisotropic conductive film in which the cationic polymerization initiator is a quaternary ammonium salt-based thermoacid generator and the cationically polymerizable component contains an alicyclic epoxy compound and a low polar oxetane compound.

また、本発明は、上述の異方性導電フィルムで、第１電子部品と第２電子部品とが異方性導電接続されている接続構造体を提供する。 The present invention also provides a connection structure in which the first electronic component and the second electronic component are anisotropically conductively connected in the above-mentioned anisotropic conductive film.

成膜用成分とカチオン重合性成分とを含有するバインダ組成物と、カチオン重合開始剤と、導電粒子とを含有する本発明の異方性導電フィルムは、カチオン重合開始剤として、第４級アンモニウム塩系熱酸発生剤を使用し、カチオン重合性成分として、脂環式エポキシ化合物と低極性オキセタン化合物とを含有している。このため、今までと変わらない硬化温度と接続信頼性とを担保しながらも、今まで以上に優れた保管ライフ性を実現できる。 The anisotropic conductive film of the present invention containing a binder composition containing a film-forming component and a cationically polymerizable component, a cationic polymerization initiator, and conductive particles is a quaternary ammonium as a cationic polymerization initiator. A salt-based thermal acid generator is used, and an alicyclic epoxy compound and a low-polarity oxetane compound are contained as cationically polymerizable components. For this reason, it is possible to realize better storage life than ever while ensuring the same curing temperature and connection reliability as before.

以下、本発明の一例を、詳細に説明する。 Hereinafter, an example of the present invention will be described in detail.

＜異方性導電フィルム＞
本発明の異方性導電フィルムは、成膜用成分とカチオン重合性成分とを含有するバインダ組成物と、カチオン重合開始剤と、導電粒子とを含有している。 <Animolic conductive film>
The anisotropic conductive film of the present invention contains a binder composition containing a film-forming component and a cationically polymerizable component, a cationic polymerization initiator, and conductive particles.

（バインダ組成物）
本発明において、導電粒子を含有保持するバインダ組成物は、成膜用成分とカチオン重合性成分とを含有している。 (Binder composition)
In the present invention, the binder composition containing and retaining the conductive particles contains a film-forming component and a cationically polymerizable component.

（成膜用成分）
成膜用成分は、異方性導電フィルムをフィルム化するために使用される成分であり、膜形成能を有する成分である。このような成膜用成分としては、フェノキシ樹脂、エポキシ樹脂、不飽和ポリエステル樹脂、飽和ポリエステル樹脂、ウレタン樹脂、ブタジエン樹脂、ポリイミド樹脂、ポリアミド樹脂、ポリオレフィン樹脂等を挙げることができ、これらの２種以上を併用することができる。これらの中でも、製膜性、加工性、接続信頼性の観点から、フェノキシ樹脂を好ましく使用することができる。 (Component for film formation)
The film-forming component is a component used for forming an anisotropic conductive film into a film, and is a component having a film-forming ability. Examples of such film-forming components include phenoxy resin, epoxy resin, unsaturated polyester resin, saturated polyester resin, urethane resin, butadiene resin, polyimide resin, polyamide resin, and polyolefin resin, and these two types can be mentioned. The above can be used together. Among these, a phenoxy resin can be preferably used from the viewpoint of film forming property, processability, and connection reliability.

バインダ組成物中の成膜用成分の配合割合は、好ましくは１０〜７０質量％、より好ましくは２０〜５０質量％である。この範囲であれば、十分なフィルム形成能を発揮することができる。 The blending ratio of the film-forming component in the binder composition is preferably 10 to 70% by mass, more preferably 20 to 50% by mass. Within this range, sufficient film forming ability can be exhibited.

（カチオン重合性成分）
カチオン重合性成分は、異方性導電フィルムを硬化させる成分であり、脂環式エポキシ化合物と低極性オキセタン化合物とを含有している。バインダ組成物中におけるカチオン重合性成分の配合量は、好ましくは１０〜８０質量％、より好ましくは２０〜６０質量％である。この範囲であれば、より高い硬化速度を有するバインダ組成物を与えることができる。 (Cationopolymerizable component)
The cationically polymerizable component is a component that cures the anisotropic conductive film, and contains an alicyclic epoxy compound and a low-polarity oxetane compound. The blending amount of the cationically polymerizable component in the binder composition is preferably 10 to 80% by mass, more preferably 20 to 60% by mass. Within this range, a binder composition having a higher curing rate can be provided.

（脂環式エポキシ化合物）
脂環式エポキシ化合物を使用する理由は、汎用のグリシジルエーテル型エポキシ化合物よりも高いその反応性を利用して、異方性導電フィルムに良好な低温速硬化性を付与するためである。このような脂環式エポキシ化合物としては、分子内に２つ以上のエポキシ基を有するものが好ましく挙げられる。これらは液状であっても、固体状であってもよい。具体的には、ジグリシジルヘキサヒドロビスフェノールＡ、３，４−エポキシシクロヘキセニルメチル−３′，４′−エポキシシクロヘキセンカルボキシレート、ジエポキシビシクロヘキシル等を挙げることができる。中でも、硬化物の光透過性を確保でき、速硬化性にも優れている点から、ジグリシジルヘキサヒドロビスフェノールＡ、中でもジエポキシビシクロヘキシルを好ましく使用することができる。 (Alicyclic epoxy compound)
The reason for using the alicyclic epoxy compound is to impart good low temperature and rapid curability to the anisotropic conductive film by utilizing its reactivity higher than that of the general-purpose glycidyl ether type epoxy compound. As such an alicyclic epoxy compound, those having two or more epoxy groups in the molecule are preferably mentioned. These may be liquid or solid. Specific examples thereof include diglycidyl hexahydrobisphenol A, 3,4-epoxycyclohexenylmethyl-3', 4'-epoxycyclohexene carboxylate, and diepoxy bicyclohexyl. Among them, diglycidyl hexahydrobisphenol A, particularly diepoxy bicyclohexyl, can be preferably used because the light transmittance of the cured product can be ensured and the quick curing property is also excellent.

（低極性オキセタン化合物）
本発明においては、脂環式エポキシ化合物に低極性オキセタン化合物を併用する。低極性オキセタン化合物は、双極子モーメントが３．０ｄ以下のオキセタン化合物であり、表面張力が比較的低く、異方性導電フィルムの膜に良好なレベリング性を付与することができ、結果的に異方性導電フィルムの保管ライフ性を向上させることが可能となる。他方、低極性オキセタン化合物は、脂環式エポキシ化合物に由来する異方性導電フィルムの示差走査熱量計（ＤＳＣ）で測定される反応開始温度と反応終了温度とを上昇させる作用を有する。このような低極性オキセタン化合物としては、３−エチル−３−（２−エチルヘキシロキシメチル）オキセタン、３−エチル−３−ヒドロキシメチルオキセタン、ジ［１−エチル（３−オキセタニル）］メチルエーテル、４，４′−ビス[（３−エチル−３−オキセタニル）メトキシメチル]ビフェニル等が挙げられる。なかでも、表面張力が低く、濡れ性に優れることから、３−エチル−３−（２−エチルヘキシロキシメチル）オキセタン、特に４，４′−ビス[（３−エチル−３−オキセタニル）メトキシメチル]ビフェニルが好ましい。 (Low-polarity oxetane compound)
In the present invention, a low-polarity oxetane compound is used in combination with the alicyclic epoxy compound. The low-polarity oxetane compound is an oxetane compound having a dipole moment of 3.0 d or less, has a relatively low surface tension, and can impart good leveling property to the film of the anisotropic conductive film, resulting in a difference. It is possible to improve the storage life of the polar conductive film. On the other hand, the low-polarity oxetane compound has an action of raising the reaction start temperature and the reaction end temperature measured by a differential scanning calorimetry (DSC) of an anisotropic conductive film derived from an alicyclic epoxy compound. Examples of such low-polarity oxetane compounds include 3-ethyl-3- (2-ethylhexyloxymethyl) oxetane, 3-ethyl-3-hydroxymethyloxetane, and di [1-ethyl (3-oxetanyl)] methyl ether. Examples thereof include 4,4'-bis [(3-ethyl-3-oxetanyl) methoxymethyl] biphenyl and the like. Among them, 3-ethyl-3- (2-ethylhexyloxymethyl) oxetane, especially 4,4'-bis [(3-ethyl-3-oxetanyl) methoxymethyl) has low surface tension and excellent wettability. ] Biphenyl is preferred.

脂環式エポキシ化合物と低極性オキセタン化合物との配合割合は、質量基準で好ましくは２５：７５〜６０：４０、より好ましくは４５：５５〜６０：４０、特に好ましくは５０：５０〜５５：４５である。この範囲よりも低極性オキセタン化合物の配合量が増加すると、反応開始温度と反応終了温度とを上昇させる傾向があり、逆に減少すると保管ライフが低下する傾向がある。従って、脂環式エポキシ化合物と低極性オキセタン化合物との配合割合を調整することにより、異方性導電フィルムの反応開始温度と反応終了温度とをコントロールすることが可能となり、更に、反応時の昇温速度等を調整することにより、反応時間をコントロールすることも可能となる。 The mixing ratio of the alicyclic epoxy compound and the low-polarity oxetane compound is preferably 25:75 to 60:40, more preferably 45:55 to 60:40, and particularly preferably 50:50 to 55:45 on a mass basis. Is. If the blending amount of the low-polarity oxetane compound is increased beyond this range, the reaction start temperature and the reaction end temperature tend to increase, and conversely, if the amount decreases, the storage life tends to decrease. Therefore, by adjusting the blending ratio of the alicyclic epoxy compound and the low-polarity oxetane compound, it is possible to control the reaction start temperature and the reaction end temperature of the anisotropic conductive film, and further, the temperature rise during the reaction. It is also possible to control the reaction time by adjusting the temperature rate and the like.

バインダ組成物は、必要に応じ、ビスフェノールＡ型エポキシ樹脂、ビスフェノールＦ型エポキシ樹脂、ノボラック型エポキシ樹脂、それらの変性エポキシ樹脂等の他のエポキシ樹脂、シランカップリング剤、充填剤、軟化剤、促進剤、老化防止剤、着色剤（顔料、染料）、有機溶剤、イオンキャッチャー剤などを含有することができる。また、必要に応じて、（メタ）アクリレート化合物とラジカル重合開始剤とを含有することができる。ここで、（メタ）アクリレート化合物としては、従来公知の（メタ）アクリレートモノマーを使用することができる。例えば、単官能（メタ）アクリレート系モノマー、二官能以上の多官能（メタ）アクリレート系モノマーを使用することができる。ここで、（メタ）アクリレートには、アクリレートとメタクリレートとが包含される。また、ラジカル重合開始剤としては、有機過酸化物、アゾビスイソブチロニトリル等の公知のラジカル重合開始剤を含有することができる。
The binder composition contains, if necessary, other epoxy resins such as bisphenol A type epoxy resin, bisphenol F type epoxy resin, novolak type epoxy resin, and their modified epoxy resins, silane coupling agents, fillers, softeners, and accelerators. It can contain agents, epoxies, colorants (pigments, dyes), organic solvents, ion catchers and the like. In addition, a (meth) acrylate compound and a radical polymerization initiator can be contained, if necessary. Here, as the (meth) acrylate compound, a conventionally known (meth) acrylate monomer can be used. For example, a monofunctional (meth) acrylate-based monomer and a bifunctional or higher polyfunctional (meth) acrylate-based monomer can be used. Here, the (meth) acrylate includes acrylate and methacrylate. As the radical polymerization initiator may contain an organic peroxide, a known radical polymerization initiator such as azobis isobutyronitrile Bed Chiro nitrile.

（導電粒子）
本発明の異方性導電フィルムは、異方性導電接続を可能とするために、バインダ組成物中に導電粒子を含有する。導電粒子としては、従来公知の異方性導電フィルムに用いられているものの中から適宜選択して使用することができる。例えばニッケル、コバルト、銀、銅、金、パラジウムなどの金属粒子、ハンダなどの合金粒子、金属被覆樹脂粒子などが挙げられる。２種以上を併用することもできる。 (Conductive particles)
The anisotropic conductive film of the present invention contains conductive particles in the binder composition in order to enable anisotropic conductive connection. As the conductive particles, those used in conventionally known anisotropic conductive films can be appropriately selected and used. Examples thereof include metal particles such as nickel, cobalt, silver, copper, gold and palladium, alloy particles such as solder, and metal-coated resin particles. Two or more types can be used together.

導電粒子の平均粒径としては、配線高さのばらつきに対応できるようにし、また、導通抵抗の上昇を抑制し、且つショートの発生を抑制するために、好ましくは２．５μｍ以上３０μｍ以下、より好ましくは３μｍ以上９μｍ以下である。導電粒子の粒径は、一般的な粒度分布測定装置により測定することができ、また、その平均粒径も粒度分布測定装置を用いて求めることができる。 The average particle size of the conductive particles is preferably 2.5 μm or more and 30 μm or less in order to cope with variations in wiring height, suppress an increase in conduction resistance, and suppress the occurrence of short circuits. It is preferably 3 μm or more and 9 μm or less. The particle size of the conductive particles can be measured by a general particle size distribution measuring device, and the average particle size thereof can also be determined by using the particle size distribution measuring device.

なお、導電粒子が金属被覆樹脂粒子である場合、樹脂コア粒子の粒子硬さ（２０％Ｋ値；圧縮弾性変形特性Ｋ２０）は、良好な接続信頼性を得るために、好ましくは１００〜１０００ｋｇｆ／ｍｍ２、より好ましくは２００から５００ｋｇｆ／ｍｍ２である。圧縮弾性変形特性Ｋ２０は、例えば、微小圧縮試験機（ＭＣＴ−Ｗ２０１、（株）島津製作所製）を使用して測定温度２０℃で測定することができる。 When the conductive particles are metal-coated resin particles, the particle hardness (20% K value; compressive elastic deformation characteristic K 20 ) of the resin core particles is preferably 100 to 1000 kgf in order to obtain good connection reliability. / Mm 2 , more preferably 200 to 500 kgf / mm 2 . The compressive elastic deformation characteristic K 20 can be measured at a measurement temperature of 20 ° C. using, for example, a microcompression tester (MCT-W201, manufactured by Shimadzu Corporation).

導電粒子の異方性導電フィルム中の存在量は、導電粒子捕捉効率の低下を抑制し、且つショートの発生を抑制するために、好ましくは１平方ｍｍ当たり５０個以上１０００００個以下、より好ましくは２００個以上７００００個以下である。この存在量の測定は材料の薄膜を光学顕微鏡で観察することにより行うことができる。なお、異方性導電接続前において、異方性導電フィルム中の導電粒子がバインダ組成物中に存在しているために光学顕微鏡で観察し難い場合がある。そのような場合には、異方性導電接続後の異方性導電フィルムを観察してもよい。この場合には、接続前後のフィルム厚変化を考慮して存在量を割り出すことができる。 The abundance of the conductive particles in the anisotropic conductive film is preferably 50 or more and 100,000 or less per square mm, more preferably 100,000 or less, in order to suppress a decrease in the conductive particle capturing efficiency and suppress the occurrence of short circuits. The number is 200 or more and 70,000 or less. This abundance can be measured by observing a thin film of the material with an optical microscope. Before the anisotropic conductive connection, the conductive particles in the anisotropic conductive film may be difficult to observe with an optical microscope because they are present in the binder composition. In such a case, the anisotropic conductive film after the anisotropic conductive connection may be observed. In this case, the abundance can be determined in consideration of the change in film thickness before and after connection.

なお、導電粒子の異方性導電フィルム中の存在量は質量基準で表すこともができる。この場合、その存在量は、異方性導電フィルムの全質量を１００質量部としたときに、その１００質量部中に好ましくは１質量部以上３０質量部以下、より好ましくは３質量部以上１０質量部以下となる量である。 The abundance of conductive particles in the anisotropic conductive film can also be expressed on a mass basis. In this case, the abundance thereof is preferably 1 part by mass or more and 30 parts by mass or less, more preferably 3 parts by mass or more and 10 parts by mass in 100 parts by mass when the total mass of the anisotropic conductive film is 100 parts by mass. The amount is less than or equal to parts by mass.

（カチオン重合開始剤）
本発明の異方性導電フィルムは、カチオン重合開始剤として、スルホニウム塩系熱酸発生剤ではなく第４級アンモニウム塩系熱酸発生剤を含有する。保管ライフ性を向上させるためである。このような第４級アンモニウム塩系熱酸発生剤としては、第４級アンモニウムカチオンと、６フッ化アンチモン酸アニオン、６フッ化リン酸アニオン、トリフルオロメタンスルホン酸アニオン、パーフルオロブタンスルホン酸アニオン、ジノニルナフタレンスルホン酸アニオン、ジノニルナフタレンスルホン酸アニオン、ｐ−トルエンスルホン酸アニオン、ドデシルベンゼンスルホン酸アニオン、またはテトラキス（ペンタフルオロフェニル）ボレートアニオンとの塩等を挙げることができる。また、第４級アンモニウムカチオンとしては、ＮＲ１Ｒ２Ｒ３Ｒ４＋で表されるカチオンを挙げることができる。ここで、Ｒ１、Ｒ２、Ｒ３及びＲ４は、直鎖、分岐鎖または環状の炭素数１〜１２のアルキル基またはアリール基であり、それぞれ水酸基、ハロゲン、アルコキシル基、アミノ基、エステル基等を有していてもよい。 (Cationic polymerization initiator)
The anisotropic conductive film of the present invention contains a quaternary ammonium salt-based thermal acid generator instead of a sulfonium salt-based thermal acid generator as a cationic polymerization initiator. This is to improve the storage life. Examples of such a quaternary ammonium salt-based thermoacid generator include a quaternary ammonium cation, an antimonic acid hexafluoride anion, a phosphate anion hexafluoride, a trifluoromethanesulfonic acid anion, and a perfluorobutanesulfonic acid anion. Examples thereof include salts with dinonylnaphthalene sulfonic acid anion, dinonylnaphthalene sulfonic acid anion, p-toluene sulfonic acid anion, dodecylbenzene sulfonic acid anion, and tetrakis (pentafluorophenyl) borate anion. Further, as the quaternary ammonium cation, a cation represented by NR1R2R3R4 + can be mentioned. Here, R1, R2, R3 and R4 are linear, branched or cyclic alkyl or aryl groups having 1 to 12 carbon atoms, and each has a hydroxyl group, a halogen, an alkoxyl group, an amino group, an ester group and the like. You may be doing it.

第４級アンモニウム塩系熱酸発生剤の具体例としては、Ｋｉｎｇ Ｉｎｄｕｓｔｒｉｅｓ，Ｉｎｃ．製造のＣＸＣ−１６１２、ＣＸＣ−１７３３、ＣＸＣ−１７３８、ＴＡＧ−２６７８、ＣＸＣ−１６１４、ＴＡＧ−２６８９、ＴＡＧ−２６９０、ＴＡＧ−２７００、ＣＸＣ−１８０２−６０、ＣＸＣ−１８２１等が挙げられる。これらは、楠本化成（株）から入手可能である。 Specific examples of the quaternary ammonium salt-based thermoacid generator include King Industries, Inc. Examples thereof include CXC-1612, CXC-1733, CXC-1738, TAG-2678, CXC-1614, TAG-2689, TAG-2690, TAG-2700, CXC-1802-60, and CXC-1821 manufactured. These are available from Kusumoto Kasei Co., Ltd.

本発明の異方性導電フィルムが、フィルムである場合、その層厚は、好ましくは３〜５０μｍ、より好ましくは５〜２０μｍである。 When the anisotropic conductive film of the present invention is a film, the layer thickness thereof is preferably 3 to 50 μm, more preferably 5 to 20 μm.

（異方性導電フィルムの製造）
本発明の異方性導電フィルムは、上述したバインダ組成物に導電粒子とカチオン重合開始剤とを、トルエン等の有機溶媒に溶解して塗料とし、その塗料を公知のフィルム化手法を利用してフィルム化することにより製造することができる。 (Manufacturing of anisotropic conductive film)
In the anisotropic conductive film of the present invention, conductive particles and a cationic polymerization initiator are dissolved in the above-mentioned binder composition in an organic solvent such as toluene to obtain a coating material, and the coating material is used as a known film-forming method. It can be produced by forming a film.

なお、本発明の異方性導電フィルムは、単層であってもよいが、異方性導電接続時の粒子捕捉性を低下させることなく、導電粒子の使用量を減じて製造コストを減少させ、且つアンダーフィル充填操作を省くために、絶縁性樹脂層を積層させてもよい。その場合、本発明の異方性導電フィルムは、導電粒子含有層／絶縁性樹脂層の２層構成となる。このような絶縁性樹脂層は、基本的には異方性導電フィルムで使用したバインダ組成物に、導電粒子を含有させることなくカチオン重合開始剤を配合させた組成物から形成することができる。 Although the anisotropic conductive film of the present invention may be a single layer, the amount of conductive particles used can be reduced to reduce the manufacturing cost without lowering the particle trapping property at the time of anisotropic conductive connection. Moreover, in order to omit the underfill filling operation, the insulating resin layer may be laminated. In that case, the anisotropic conductive film of the present invention has a two-layer structure of a conductive particle-containing layer / an insulating resin layer. Such an insulating resin layer can be basically formed from a composition in which a cationic polymerization initiator is blended with the binder composition used in the anisotropic conductive film without containing conductive particles.

本発明の異方性導電フィルムは、反応速度コントロールとの観点から、示差走査熱量計で測定した反応ピークの反応開始温度を６０〜８０℃に調整し、また、反応終了温度を１５５〜１８５℃に調整することが好ましい。これらの調整は、脂環式エポキシ化合物と低極性オキセタン化合物との配合割合を調整すること等により行うことができる。 From the viewpoint of controlling the reaction rate, the anisotropic conductive film of the present invention adjusts the reaction start temperature of the reaction peak measured by a differential scanning calorimeter to 60 to 80 ° C. and sets the reaction end temperature to 155 to 185 ° C. It is preferable to adjust to. These adjustments can be made by adjusting the blending ratio of the alicyclic epoxy compound and the low-polarity oxetane compound.

＜接続構造体＞
本発明の異方性導電フィルムは、ＩＣチップ、ＩＣモジュール、ＦＰＣなどの第１電子部品と、プラスチック基板、ガラス基板、リジッド基板、セラミック基板、ＦＰＣなどの第２電子部品とを異方性導電接続する際に好ましく適用することができる。このような本発明の異方性導電フィルムで、第１電子部品と第２電子部品とが異方性導電接続されている接続構造体も本発明の一部である。なお、異方性導電フィルムを用いた電子部品の接続方法としては、公知の手法を利用することができる。 <Connection structure>
The anisotropic conductive film of the present invention is anisotropic conductive between a first electronic component such as an IC chip, an IC module and an FPC and a second electronic component such as a plastic substrate, a glass substrate, a rigid substrate, a ceramic substrate and an FPC. It can be preferably applied when connecting. In such an anisotropic conductive film of the present invention, a connection structure in which the first electronic component and the second electronic component are anisotropically conductively connected is also a part of the present invention. As a method for connecting electronic components using an anisotropic conductive film, a known method can be used.

以下、本発明を実施例により具体的に説明する。 Hereinafter, the present invention will be specifically described with reference to Examples.

実施例１
（導電粒子含有層の形成）
フェノキシ樹脂（ＹＰ−５０、新日鉄住金化学（株））６０質量部、脂環式エポキシ化合物としてジエポキシビシクロヘキシル（セロキサイド８０００、（株）ダイセル）１０質量部、低極性オキセタン化合物（ＯＸＢＰ、宇部興産（株））２０質量部、熱カチオン重合開始剤（第４級アンモニウム塩系熱酸発生剤、商品名ＣＸＣ−１６１２、楠本化成（株））２質量部、および平均粒径３μｍの導電性粒子（Ｎｉ／Ａｕメッキ樹脂粒子、ＡＵＬ７０４、積水化学工業（株））５０質量部を、トルエンに添加し、固形分が５０質量％となるよう混合液を調製した。 Example 1
(Formation of conductive particle-containing layer)
Phenoxy resin (YP-50, Nippon Steel & Sumikin Chemical Co., Ltd.) 60 parts by mass, diepoxybicyclohexyl (celloxide 8000, Daicel Co., Ltd.) 10 parts by mass as an alicyclic epoxy compound, low polar oxetane compound (OXBP, Ube Kosan) (Co., Ltd.) 20 parts by mass, thermal cationic polymerization initiator (quaternary ammonium salt-based thermoacid generator, trade name CXC-1612, Kusumoto Kasei Co., Ltd.) 2 parts by mass, and conductive particles having an average particle size of 3 μm (Ni / Au plated resin particles, AUL704, Sekisui Chemical Industry Co., Ltd.) 50 parts by mass was added to toluene to prepare a mixed solution so that the solid content was 50% by mass.

得られた混合液を、厚さ５０μｍのポリエチレンテレフタレート剥離フィルム（ＰＥＴ剥離フィルム）上に、乾燥厚が６μｍとなるよう塗布し、６０℃のオーブン中で５分間乾燥することにより、導電粒子含有層を形成した。 The obtained mixed solution was applied onto a polyethylene terephthalate release film (PET release film) having a thickness of 50 μm so as to have a drying thickness of 6 μm, and dried in an oven at 60 ° C. for 5 minutes to obtain a conductive particle-containing layer. Was formed.

（絶縁性樹脂層の形成）
導電粒子を用いない以外は、導電粒子含有層の形成の際に使用した原材料と同じ原材料をトルエンに添加し、固形分が５０質量％となるよう混合液を調製した。 (Formation of insulating resin layer)
The same raw material as the raw material used for forming the conductive particle-containing layer was added to toluene except that conductive particles were not used, and a mixed solution was prepared so that the solid content was 50% by mass.

得られた混合液を、厚さ５０μｍのＰＥＴ剥離フィルム上に、乾燥厚が１２μｍとなるよう塗布し、６０℃のオーブン中で５分間乾燥することにより、絶縁性樹脂層を形成した。 The obtained mixed solution was applied onto a PET release film having a thickness of 50 μm so as to have a drying thickness of 12 μm, and dried in an oven at 60 ° C. for 5 minutes to form an insulating resin layer.

（異方性導電フィルムの作成）
導電粒子含有層に絶縁性樹脂層を、６０℃、５ＭＰａでラミネー卜することにより、厚さ５０μｍの一対のＰＥＴ剥離フィルムで挟持された異方性導電フィルムを得た。 (Creation of anisotropic conductive film)
An insulating resin layer was laminated on the conductive particle-containing layer at 60 ° C. and 5 MPa to obtain an anisotropic conductive film sandwiched between a pair of PET release films having a thickness of 50 μm.

実施例２〜４
導電粒子含有層および絶縁性樹脂層における脂環式エポキシ化合物（セロキサイド８０００、（株）ダイセル）と低極性オキセタン化合物として４，４′−ビス[（３−エチル−３−オキセタニル）メトキシメチル]ビフェニル（０ＸＢＰ、宇部興産（株））との配合量（比率）を、表１に示すように変更した以外は、実施例１と同様に異方性導電フィルムを得た。 Examples 2-4
Alicyclic epoxy compounds (celloxide 8000, Daicel Co., Ltd.) and 4,4'-bis [(3-ethyl-3-oxetanyl) methoxymethyl] biphenyl as low-polarity oxetane compounds in the conductive particle-containing layer and the insulating resin layer An anisotropic conductive film was obtained in the same manner as in Example 1 except that the compounding amount (ratio) with (0XBP, Ube Kosan Co., Ltd.) was changed as shown in Table 1.

比較例１〜４
導電粒子含有層および絶縁性樹脂層における熱カチオン重合開始剤を、表１に示すようにスルホニウム塩系熱酸発生剤（ＳＩ−６０Ｌ、三新化学工業（株））に代えた以外は、実施例１〜４と同様に異方性導電フィルムを作成した。 Comparative Examples 1 to 4
Implemented except that the thermal cationic polymerization initiator in the conductive particle-containing layer and the insulating resin layer was replaced with a sulfonium salt-based thermal acid generator (SI-60L, Sanshin Chemical Industry Co., Ltd.) as shown in Table 1. An anisotropic conductive film was prepared in the same manner as in Examples 1 to 4.

実施例５〜１３、比較例５
導電粒子含有層及び絶縁性樹脂層における脂環式エポキシ化合物（セロキサイド８０００、（株）ダイセル）と低極性オキセタン化合物（０ＸＢＰ、宇部興産（株））との配合量（比率）を、表１に示すよう変更した以外は、実施例１と同様に異方性導電フィルムを作成した。 Examples 5 to 13, Comparative Example 5
Table 1 shows the blending amounts (ratio) of the alicyclic epoxy compound (Ceroxide 8000, Daicel Co., Ltd.) and the low-polarity oxetane compound (0XBP, Ube Kosan Co., Ltd.) in the conductive particle-containing layer and the insulating resin layer. An anisotropic conductive film was prepared in the same manner as in Example 1 except that the changes were made as shown.

＜＜評価＞＞
各実施例及び比較例で得られた異方性導電フィルムについて、以下に説明するように「保管ライフ特性」、「硬化温度」、「密着特性」及び「反応時間」を試験もしくは測定し、評価した。 << Evaluation >>
For the anisotropic conductive films obtained in each Example and Comparative Example, "storage life characteristics", "curing temperature", "adhesion characteristics" and "reaction time" are tested or measured and evaluated as described below. did.

＜保管ライフ特性＞
一対のＰＥＴ剥離フィルムに挟持されている異方性導電フィルムを、湿度４０％、温度２５℃又は３０℃に設定されている恒温恒湿室に投入し、投入後２４時間毎にサンプリングを行い、以下の仮張り評価および圧着評価を実施し、それらの評価結果から総合的に保管ライフ特性を評価した。得られた結果を表１に示す。 <Storage life characteristics>
The anisotropic conductive film sandwiched between the pair of PET release films is placed in a constant temperature and humidity chamber set to a humidity of 40% and a temperature of 25 ° C. or 30 ° C., and sampling is performed every 24 hours after the injection. The following temporary tension evaluation and crimping evaluation were carried out, and the storage life characteristics were comprehensively evaluated from the evaluation results. The results obtained are shown in Table 1.

（仮張り評価）
異方性導電フィルムの導電粒子含有層側のＰＥＴ剥離フィルムを剥離し、導電粒子含有層側から異方性導電フィルムを素ガラスに貼り付け、素ガラスと異方性導電フィルムとの積層体を作製した。この積層体をその素ガラス側が４５℃に設定したホットプレートに接触するように載置し、異方性導電フィルム側から手で圧力をかけ、その後、室温にまで冷却した。冷却後、積層体から絶縁性樹脂層側のＰＥＴ剥離フィルムを剥がし、素ガラスから異方性導電フィルムが剥がれることなく、ＰＥＴ剥離フィルムだけが剥がれるか否かを確認した。 (Temporary tension evaluation)
The PET release film on the conductive particle-containing layer side of the anisotropic conductive film is peeled off, the anisotropic conductive film is attached to the base glass from the conductive particle-containing layer side, and the laminate of the base glass and the anisotropic conductive film is formed. Made. The laminate was placed so that its raw glass side was in contact with a hot plate set at 45 ° C., pressure was manually applied from the anisotropic conductive film side, and then the mixture was cooled to room temperature. After cooling, the PET release film on the insulating resin layer side was peeled off from the laminate, and it was confirmed whether or not only the PET release film could be peeled off without peeling off the anisotropic conductive film from the raw glass.

（圧着評価）
テスト用ＩＣチップとテスト用基板との間に、ＩＣチップ側に絶縁性樹脂層が配置されるよう異方性導電フィルムを挟み、加熱加圧（１２０℃、６０ＭＰａ、５秒）し、評価用接続物を作成した。作成した接続物の圧痕状態を確認し、圧痕が薄くならず、消失せずに残存するかを確認した。 (Crimping evaluation)
An anisotropic conductive film is sandwiched between the test IC chip and the test substrate so that an insulating resin layer is arranged on the IC chip side, and heated and pressurized (120 ° C., 60 MPa, 5 seconds) for evaluation. I made a connection. The indentation state of the created connection was confirmed, and it was confirmed whether the indentation did not become thin and remained without disappearing.

（保管ライフ特性評価）
仮張り評価において、素ガラスから異方性導電フィルムが剥がれた時点を保管ライフとした。また、仮張り評価において、素ガラスから異方性導電フィルムが剥がれなかった場合でも、圧着評価において、圧痕が薄くなった（消失した）時点を保管ライフとした。 (Evaluation of storage life characteristics)
In the temporary tension evaluation, the time when the anisotropic conductive film was peeled off from the raw glass was defined as the storage life. Further, even when the anisotropic conductive film was not peeled off from the raw glass in the temporary tension evaluation, the time when the indentation became thin (disappeared) in the crimping evaluation was defined as the storage life.

＜硬化温度＞
テスト用ＩＣチップとテスト用基板との間に、ＩＣチップ側に絶縁性樹脂層が配置されるよう異方性導電フィルムを挟み、加熱加圧（８０℃、９０℃、１００℃、１１０℃、又は１２０℃、６０ＭＰａ、５秒）し、評価用接続物を得た。この接続物における異方性導電フィルムの反応率を以下に説明するように測定し、その測定結果から硬化温度を決定した。得られた結果を表１に示す。 <Curing temperature>
An anisotropic conductive film is sandwiched between the test IC chip and the test substrate so that an insulating resin layer is arranged on the IC chip side, and heat and pressure (80 ° C, 90 ° C, 100 ° C, 110 ° C, Alternatively, the temperature was 120 ° C., 60 MPa, 5 seconds) to obtain an evaluation connector. The reaction rate of the anisotropic conductive film in this connection was measured as described below, and the curing temperature was determined from the measurement results. The results obtained are shown in Table 1.

（反応率測定）
評価用接続物のＩＣチップを手で摘まんで剥がし、硬化した異方性導電フィルムを露出させ、異方性導電フィルムをサンプリングした。得られたサンプルを、濃度０．１ｇ／ｍＬとなるようアセトニトリルに溶解した。別途、硬化前の異方性導電フィルムを同様の濃度となるようアセトニトリルに溶解し、ＨＰＬＣ−ＭＳ（ＷａｔｅｒＳ社製）を用いて、以下の条件にて各モノマーのピーク強度を確認した。硬化後のピーク強度の減少量より各温度での反応率を求め、反応率８０％以上となる温度を、硬化温度とした。 (Measurement of reaction rate)
The IC chip of the evaluation connection was picked and peeled off by hand to expose the cured anisotropic conductive film, and the anisotropic conductive film was sampled. The obtained sample was dissolved in acetonitrile to a concentration of 0.1 g / mL. Separately, the anisotropic conductive film before curing was dissolved in acetonitrile so as to have the same concentration, and the peak intensity of each monomer was confirmed under the following conditions using HPLC-MS (manufactured by WaterS). The reaction rate at each temperature was determined from the amount of decrease in peak intensity after curing, and the temperature at which the reaction rate was 80% or more was defined as the curing temperature.

溶媒：水／アセ卜ニトリル混合溶液（９０／１０）６０質量部に、アセトニトリル４０質量部を混合した混合溶媒
流量：０．４ｍＬ／ｍｉｎ
カラム：１０ｃｍ、４０℃Ｃ
注入量：５μＬ
解析波：２１０−４１０ｎｍ Solvent: A mixed solvent in which 40 parts by mass of acetonitrile is mixed with 60 parts by mass of a mixed solution of water / acetylnitrile (90/10) Flow rate: 0.4 mL / min
Column: 10 cm, 40 ° C C
Injection volume: 5 μL
Analysis wave: 210-410 nm

＜密着特性＞
テスト用ＩＣチップとテスト用基板との間に、ＩＣチップ側に絶縁性樹脂層が配置されるよう異方性導電フィルムを挟み、加熱加圧（１２０℃、６０ＭＰａ、５秒）し、評価用接続物を得た。この接続物に対して、エタック社製、型式ＥＨＳ−４１１Ｍを用いて、プレッシャークッカーテスト（ＰＣＴ）を実施した。具体的には、得られた評価用接続物を、１２１℃、２ａｔｍ、飽和水蒸気雰囲気という条件に設定された恒温恒湿槽に接続物を投入し、２４時間毎に以下の密着評価を行った。得られた結果を表１に示す。 <Adhesion characteristics>
An anisotropic conductive film is sandwiched between the test IC chip and the test substrate so that the insulating resin layer is arranged on the IC chip side, and heated and pressurized (120 ° C., 60 MPa, 5 seconds) for evaluation. I got a connection. A pressure cooker test (PCT) was carried out on this connection using a model EHS-411M manufactured by Etac. Specifically, the obtained evaluation connection was put into a constant temperature and humidity chamber set under the conditions of 121 ° C., 2 atm, and a saturated steam atmosphere, and the following adhesion evaluation was performed every 24 hours. .. The results obtained are shown in Table 1.

（密着評価）
ＰＣＴ試験に投入した接続物の外観確認を行い、異方性導電フィルムとＩＣチップもしく基板との層間で剥離が生じているかを目視観察した。
ランク 基準
〇： ＩＣ圧着後、４８時間のＰＣＴでも剥離が観察されない場合
△： ＩＣ圧着後、２４時間のＰＣＴでは剥離が観察されないが、４８時間のＰＣＴ試験では剥離が観察された場合
×： ＩＣ圧着後、ＰＣＴを行う前にすでに剥離が観察されていたか、２４時間のＰＣＴで剥離が観察された場合 (Adhesion evaluation)
The appearance of the connected object put into the PCT test was confirmed, and it was visually observed whether peeling occurred between the anisotropic conductive film and the IC chip or the substrate.
Rank Criteria 〇: When peeling is not observed even in PCT for 48 hours after IC crimping Δ: When peeling is not observed in PCT for 24 hours after IC crimping, but peeling is observed in PCT test for 48 hours ×: IC If peeling has already been observed after crimping and before PCT, or if peeling has been observed after 24 hours of PCT.

＜反応時間＞
得られた異方性導電フィルムから切り出した約５ｍｇのサンプルを、アルミＰＡＮ（ＴＡ Ｉｎｓｔｒｕｍｅｎｔｓ Ｉｎｃ．）に格納し、それをＤＳＣ測定装置（Ｑ２０００，ＴＡ Ｉｎｓｔｒｕｍｅｎｔｓ Ｉｎｃ．）にセットし、３０℃から２５０℃まで、１０℃／分の昇温速度で示差走査熱量計（ＤＳＣ）測定を行った。得られたＤＳＣチャートから、発熱ピークが立ち上がった時点の温度を反応開始温度として読み取り、発熱ピークがベースラインに変化した時点の温度を反応終了温度として読み取った。また、反応時間を以下の式に従って算出した。得られた結果を表１に示す。 <Reaction time>
About 5 mg of a sample cut out from the obtained anisotropic conductive film was stored in an aluminum PAN (TA Instruments Inc.), set in a DSC measuring device (Q2000, TA Instruments Inc.), and set at 30 ° C. to 250 ° C. Differential scanning calorimetry (DSC) measurements were performed up to ° C. at a heating rate of 10 ° C./min. From the obtained DSC chart, the temperature at the time when the exothermic peak rose was read as the reaction start temperature, and the temperature at the time when the exothermic peak changed to the baseline was read as the reaction end temperature. The reaction time was calculated according to the following formula. The results obtained are shown in Table 1.

Figure 0006776609
Figure 0006776609

Figure 0006776609
Figure 0006776609

＜＜評価結果の考察＞＞
表１の結果（実施例１と比較例１との対比、実施例２と比較例２との対比、実施例３と比較例３との対比、実施例４と比較例４との対比）から、スルホニウム塩系熱酸発生剤に代えて第４級アンモニウム塩系熱酸発生剤を使用すると、脂環式エポキシ化合物と低極性オキセタン化合物との間の配合比に変動があっても、硬化温度や接続信頼性の評価指標となる密着特性を変化させずに保管ライフを大きく向上させ得ることがわかる。 << Consideration of evaluation results >>
From the results of Table 1 (comparison between Example 1 and Comparative Example 1, comparison between Example 2 and Comparative Example 2, comparison between Example 3 and Comparative Example 3, comparison between Example 4 and Comparative Example 4). , When a quaternary ammonium salt-based thermoacid generator is used instead of the sulfonium salt-based thermoacid generator, the curing temperature is changed even if the compounding ratio between the alicyclic epoxy compound and the low-polarity oxetane compound varies. It can be seen that the storage life can be greatly improved without changing the adhesion characteristics, which is an evaluation index of connection reliability.

また、実施例１、５〜７及び比較例５の対比から、脂環式エポキシ化合物に対して低極性オキセタン化合物の配合割合が増加するにつれ、保管ライフが向上する傾向があるが、相対的に脂環式エポキシ化合物の配合量が減少すると密着特性が低下する傾向があることがわかる。逆に、実施例８〜１３の対比から、脂環式エポキシ化合物に対して低極性オキセタン化合物の配合割合が減少するにつれ、保管ライフが低下する傾向があることがわかる。 Further, from the comparison of Examples 1, 5 to 7 and Comparative Example 5, the storage life tends to be improved as the blending ratio of the low polar oxetane compound with respect to the alicyclic epoxy compound increases, but relatively It can be seen that the adhesion characteristics tend to decrease as the amount of the alicyclic epoxy compound is reduced. On the contrary, from the comparison of Examples 8 to 13, it can be seen that the storage life tends to decrease as the blending ratio of the low-polarity oxetane compound with respect to the alicyclic epoxy compound decreases.

なお、実施例１、実施例５〜１３、比較例５において行ったＤＳＣ測定結果の対比から、低極性オキセタン化合物の配合量が増加すると、反応開始温度と反応終了温度とを上昇させる傾向があることが分かる。 From the comparison of the DSC measurement results performed in Examples 1, 5 to 13 and Comparative Example 5, when the blending amount of the low-polarity oxetane compound increases, the reaction start temperature and the reaction end temperature tend to increase. You can see that.

脂環式エポキシ化合物を使用するカチオン重合性の本発明の異方性導電フィルムは、スルホニウム塩系熱酸発生剤を使用した従来の異方性導電フィルムと同等の硬化温度と接続信頼性とを担保しながらも、今まで以上に優れた保管ライフ性を実現できるので、ＩＣチップなどの電子部品の配線基板への異方性導電接続に有用である。 The cationically polymerizable anisotropic conductive film of the present invention using the alicyclic epoxy compound has the same curing temperature and connection reliability as the conventional anisotropic conductive film using a sulfonium salt-based thermal acid generator. While ensuring, it is possible to realize better storage life than ever before, which is useful for anisotropic conductive connection of electronic components such as IC chips to wiring boards.

Claims (13)

成膜用成分とカチオン重合性成分とを含有するバインダ組成物と、カチオン重合開始剤と、導電粒子とを含有する異方性導電フィルムであって、
カチオン重合開始剤が、第４級アンモニウム塩系熱酸発生剤であり、カチオン重合性成分が、脂環式エポキシ化合物と低極性オキセタン化合物とを含有しており、
以下で定義される保管ライフ特性が５日以上であり、４５℃で仮貼り性を満足する異方性導電フィルム；
＜保管ライフ特性＞
一対の剥離フィルムに挟持されている異方性導電フィルムを、湿度４０％、温度２５℃又は３０℃に設定されている恒温恒湿室に投入し、投入後２４時間毎にサンプリングを行い、以下の仮張り評価および圧着評価を実施し、それらの評価結果から保管ライフ特性を評価する；
（仮張り評価）
異方性導電フィルムの導電粒子含有層側の剥離フィルムを剥離し、導電粒子含有層側から異方性導電フィルムをガラスに貼り付け、ガラスと異方性導電フィルムとの積層体を作製し、この積層体をそのガラス側が４５℃に設定したホットプレートに接触するように載置し、異方性導電フィルム側から手で圧力をかけ、その後、室温にまで冷却し、冷却後、積層体から絶縁性樹脂層側の剥離フィルムを剥がし、ガラスから異方性導電フィルムが剥がれることなく、剥離フィルムだけが剥がれるか否かを確認する；
（圧着評価）
テスト用ＩＣチップとテスト用基板との間に、ＩＣチップ側に絶縁性樹脂層が配置されるよう異方性導電フィルムを挟み、加熱加圧（１２０℃、６０ＭＰａ、５秒）し、評価用接続物を作成し、作成した接続物の圧痕状態を確認し、圧痕が薄くならず、消失せずに残存するかを確認する；
（保管ライフ特性評価）
仮張り評価において、ガラスから異方性導電フィルムが剥がれた時点、又は仮張り評価において、ガラスから異方性導電フィルムが剥がれなかった場合でも、圧着評価において、圧痕が薄くなった（消失した）時点を保管ライフとする。 An anisotropic conductive film containing a binder composition containing a film-forming component and a cationically polymerizable component, a cationic polymerization initiator, and conductive particles.
The cationic polymerization initiator is a quaternary ammonium salt-based thermal acid generator, and the cationically polymerizable component contains an alicyclic epoxy compound and a low-polarity oxetane compound.
An anisotropic conductive film having a storage life characteristic of 5 days or more and satisfying temporary stickability at 45 ° C. as defined below ;
<Storage life characteristics>
The anisotropic conductive film sandwiched between the pair of release films is put into a constant temperature and humidity chamber set to a humidity of 40% and a temperature of 25 ° C. or 30 ° C., and sampling is performed every 24 hours after the introduction. Temporary tension evaluation and crimping evaluation are carried out, and the storage life characteristics are evaluated from those evaluation results;
(Temporary tension evaluation)
The release film on the conductive particle-containing layer side of the anisotropic conductive film is peeled off, and the anisotropic conductive film is attached to the glass from the conductive particle-containing layer side to prepare a laminate of the glass and the anisotropic conductive film. This laminate is placed so that its glass side is in contact with a hot plate set at 45 ° C., pressure is applied by hand from the anisotropic conductive film side, then cooled to room temperature, cooled, and then from the laminate. Peel off the release film on the insulating resin layer side, and check whether only the release film can be peeled off without peeling off the anisotropic conductive film from the glass;
(Crimping evaluation)
An anisotropic conductive film is sandwiched between the test IC chip and the test substrate so that an insulating resin layer is arranged on the IC chip side, and heated and pressurized (120 ° C., 60 MPa, 5 seconds) for evaluation. Create a connection, check the indentation state of the created connection, and check if the indentation does not become thin and remains without disappearing;
(Evaluation of storage life characteristics)
Even when the anisotropic conductive film was peeled off from the glass in the temporary tension evaluation, or even when the anisotropic conductive film was not peeled off from the glass in the temporary tension evaluation, the indentation became thin (disappeared) in the crimp evaluation. The time point is the storage life. 脂環式エポキシ化合物と低極性オキセタン化合物との配合割合が、質量基準で２５：７５〜６０：４０である請求項１記載の異方性導電フィルム。 The anisotropic conductive film according to claim 1, wherein the compounding ratio of the alicyclic epoxy compound and the low-polarity oxetane compound is 25:75 to 60:40 on a mass basis. 脂環式エポキシ化合物と低極性オキセタン化合物との配合割合が、質量基準で４５：５５〜６０：４０である請求項１記載の異方性導電フィルム。 The anisotropic conductive film according to claim 1, wherein the compounding ratio of the alicyclic epoxy compound and the low-polarity oxetane compound is 45:55 to 60:40 on a mass basis. 第４級アンモニウム塩系熱酸発生剤が、第４級アンモニウムカチオンと、６フッ化アンチモン酸アニオン、６フッ化リン酸アニオン、トリフルオロメタンスルホン酸アニオン、パーフルオロブタンスルホン酸アニオン、ジノニルナフタレンスルホン酸アニオン、ジノニルナフタレンスルホン酸アニオン、ｐ−トルエンスルホン酸アニオン、ドデシルベンゼンスルホン酸アニオン、またはテトラキス（ペンタフルオロフェニル）ボレートアニオンとの塩である請求項１〜３のいずれかに記載の異方性導電フィルム。 The quaternary ammonium salt-based thermoacid generators are quaternary ammonium cations, hexafluorinated antimonate anion, hexafluorinated phosphate anion, trifluoromethanesulfonic acid anion, perfluorobutane sulfonic acid anion, and dinonylnaphthalene sulfone. The variant according to any one of claims 1 to 3, which is a salt with an acid anion, a dinonylnaphthalene sulfonate anion, a p-toluene sulfonic acid anion, a dodecylbenzene sulfonic acid anion, or a tetrakis (pentafluorophenyl) borate anion. Sexual conductive film. 第４級アンモニウムカチオンが、ＮＲ１Ｒ２Ｒ３Ｒ４+で表されるカチオンであり、Ｒ１、Ｒ２、Ｒ３及びＲ４は、直鎖、分岐鎖または環状の炭素数１〜１２のアルキル基またはアリール基である請求項４記載の異方性導電フィルム。 Claim 4 in which the quaternary ammonium cation is a cation represented by NR1R2R3R4 + , and R1, R2, R3 and R4 are linear, branched or cyclic alkyl or aryl groups having 1 to 12 carbon atoms. The anisotropic conductive film according to the above. 脂環式エポキシ化合物が、ジグリシジルヘキサヒドロビスフェノールＡ又はジエポキシビシクロヘキシルであり、低極性オキセタン化合物が、３−エチル−３−（２−エチルヘキシロキシメチル）オキセタン又は４，４′−ビス[（３−エチル−３−オキセタニル）メトキシメチル]ビフェニルである請求項１〜５のいずれかに記載の異方性導電フィルム。 The alicyclic epoxy compound is diglycidyl hexahydrobisphenol A or diepoxybicyclohexyl, and the low polar oxetane compound is 3-ethyl-3- (2-ethylhexyloxymethyl) oxetane or 4,4'-bis [ The anisotropic conductive film according to any one of claims 1 to 5, which is (3-ethyl-3-oxetanyl) methoxymethyl] biphenyl. 成膜用成分がフェノキシ樹脂である請求項１〜６のいずれかに記載の異方性導電フィルム。 The anisotropic conductive film according to any one of claims 1 to 6, wherein the film-forming component is a phenoxy resin. 示差走査熱量計で測定した反応ピークの反応開始温度が６０〜８０℃であり、反応終了温度が１５５〜１８５℃である請求項１〜７のいずれかに記載の異方性導電フィルム。 The anisotropic conductive film according to any one of claims 1 to 7, wherein the reaction start temperature of the reaction peak measured by the differential scanning calorimeter is 60 to 80 ° C., and the reaction end temperature is 155 to 185 ° C. 更に、絶縁性樹脂層が積層されている請求項１〜８のいずれかに記載の異方性導電フィルム。 The anisotropic conductive film according to any one of claims 1 to 8, wherein an insulating resin layer is laminated. 導電粒子が、金属粒子、合金粒子又は金属被覆樹脂粒子である請求項１〜９のいずれかに記載の異方性導電フィルム。 The anisotropic conductive film according to any one of claims 1 to 9, wherein the conductive particles are metal particles, alloy particles, or metal-coated resin particles. 導電粒子が２種以上の導電粒子を併用している請求項１〜１０のいずれかに記載の異方性導電フィルム。 The anisotropic conductive film according to any one of claims 1 to 10, wherein two or more kinds of conductive particles are used in combination. 請求項１〜１１のいずれかに記載の異方性導電フィルムで、第１電子部品と第２電子部品とが異方性導電接続されている接続構造体。 The anisotropic conductive film according to any one of claims 1 to 11, wherein the first electronic component and the second electronic component are anisotropically conductively connected. 請求項１〜１１のいずれかに記載の異方性導電フィルムで、第１電子部品と第２電子部品とを異方性導電接続する、接続構造体の製造方法。 A method for manufacturing a connection structure, wherein the anisotropic conductive film according to any one of claims 1 to 11 is used to connect the first electronic component and the second electronic component anisotropically and conductively.
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